Abstract
Analysis of samples in the liquid environment using X-ray spectroscopy techniques is a very attractive approach as it provides specimen characterization in its native conditions thanks to the penetrating properties of X-rays. However, very often due to challenging synthesis procedures and the high cost of specimens it is difficult to obtain a sample in quantities for optimal measurement. Additionally, nanoparticles (NPs) aqueous suspensions are often not stable and undergo agglomeration and sedimentation processes that can be avoided either by sonication or sample stirring. Relatively small sample volumes and intrinsic agglomeration processes make X-ray spectroscopy measurements challenging especially when long periods are needed for the collection of high-quality data. To address both issues, we developed dedicated sample system that allows measurements down to few tens of μL of the liquid sample with capability of continuous stirring of the suspension. The X-ray spectroscopy measurements of ZnO nanoparticles suspension in water showed a stable signal for hours of acquisition time. On the other hand, in the absence of stirring, agglomeration and subsequent sedimentation processes were visible already within few minutes with maximum sedimentation rate of 2.5% of concentration loss in the beam field per minute.
Highlights
Nanotechnology is a very rapidly growing multidisciplinary field of science applied in numerous areas both at the high-tech and generalpurpose level [1,2]
To address issues associated with the examination of nanostructures in solutions, we report a recently developed microliter-stirred sample setup designed to characterize very low amounts of nano material suspensions of down to 50 μL with sustained sample mixing successfully preventing particle agglomeration and sedimentation
We presented the newly developed microliter-stirred sample setup designed to allow examination of down to 50 μL of liquid nanomaterial suspensions with continuous mixing of the sample during measurement preventing its agglomeration and subse quent sedimentation
Summary
Nanotechnology is a very rapidly growing multidisciplinary field of science applied in numerous areas both at the high-tech and generalpurpose level [1,2] It focuses on nanomaterials typically defined as objects with characteristic dimensions below 100 nm whose sizedependent properties are driven by quantum phenomenons [3]. Most of the commercially available laboratory instruments intended for the analysis of liquid samples are not adapted for continuous mixing of low sample volumes Such a system should provide a sufficient amount of space as well as accessibility in the immediate sample environment allowing to implement X-ray spectroscopy methods to probe the nanomaterial. To address issues associated with the examination of nanostructures in solutions, we report a recently developed microliter-stirred sample setup designed to characterize very low amounts of nano material suspensions of down to 50 μL with sustained sample mixing successfully preventing particle agglomeration and sedimentation. We demonstrate that the use of X-ray spectroscopy allows for in situ, element-specific, quantita tive investigations of ZnO NPs and determination of NPs agglomeration and sedimentation rates
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